CN117487546A - Green preparation method of adjustable double-emission carbon quantum dots - Google Patents
Green preparation method of adjustable double-emission carbon quantum dots Download PDFInfo
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000008367 deionised water Substances 0.000 claims abstract description 18
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000001514 detection method Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 238000003763 carbonization Methods 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000000605 extraction Methods 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- 241001122767 Theaceae Species 0.000 claims abstract 5
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 22
- 239000012046 mixed solvent Substances 0.000 abstract description 4
- 231100000956 nontoxicity Toxicity 0.000 abstract description 3
- 238000000295 emission spectrum Methods 0.000 description 23
- 230000005284 excitation Effects 0.000 description 13
- 244000269722 Thea sinensis Species 0.000 description 12
- 230000003595 spectral effect Effects 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 235000013616 tea Nutrition 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000000862 absorption spectrum Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 235000009569 green tea Nutrition 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 235000006468 Thea sinensis Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002902 bimodal effect Effects 0.000 description 1
- 235000020279 black tea Nutrition 0.000 description 1
- DEGAKNSWVGKMLS-UHFFFAOYSA-N calcein Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC(CN(CC(O)=O)CC(O)=O)=C(O)C=C1OC1=C2C=C(CN(CC(O)=O)CC(=O)O)C(O)=C1 DEGAKNSWVGKMLS-UHFFFAOYSA-N 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000007833 carbon precursor Substances 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000001748 luminescence spectrum Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 229960002378 oftasceine Drugs 0.000 description 1
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- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000020334 white tea Nutrition 0.000 description 1
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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Abstract
The invention discloses a green preparation method of an adjustable double-emission carbon quantum dot, which is characterized by comprising the following steps: (1) Grinding tea into powder, extracting with absolute ethanol as extraction solvent, filtering to remove tea residue, and collecting extractive solution; (2) Mixing a certain amount of extracting solution with deionized water to make the volume content of the deionized water in the mixed solution be 10% -80%, transferring the mixed solution into a reaction kettle, performing hydrothermal carbonization, and naturally cooling to room temperature after the reaction is finished; (3) And centrifuging and filtering the obtained product to obtain a double-emission carbon quantum dot solution, and storing the double-emission carbon quantum dot solution at the temperature of 4 ℃ for standby. The invention can realize the adjustable and controllable dual-peak emission intensity by simply changing the water content in the mixed solvent. The method has the characteristics of green and environment-friendly process, no toxicity, low cost, simple operation and the like, and can be widely applied to the fields of photoelectric devices, ion detection, temperature sensing and the like.
Description
Technical Field
The invention belongs to the field of preparation of fluorescent nano materials, and particularly relates to a green preparation method of adjustable double-emission carbon quantum dots.
Background
The carbon quantum dots (Carbon Quantum Dots, CQDs) are fluorescent nano materials composed of a carbonaceous framework with the size smaller than 10nm and surface groups, and have the advantages of low cost, environment friendliness, wide raw material sources, high biocompatibility, stable optical performance, easiness in surface modification and the like. The advantages lead the sensor to have wide application prospect in the fields of sensing, imaging, detection, catalysis, display and the like.
Methods for preparing carbon quantum dots can be divided into two main types according to different raw materials: top-down (Top-down) and Bottom-up (Bottom-up) methods, wherein the Top-down method is to destroy and disperse large-size carbon precursors into small-size carbon quantum dots by a physical or chemical method, and the raw materials mainly comprise graphite, carbon nanotubes, activated carbon, candle ash and the like; the bottom-up rule mainly refers to polymerizing and carbonizing a series of small molecules into carbon quantum dots through chemical reaction, and most of raw materials are biomass or organic small molecules; among them, the bottom-up method is the most commonly used method in the synthesis of carbon quantum dots, and includes combustion method, template method, pyrolysis method, microwave method, hydrothermal method, etc.
At present, most reported carbon quantum dots are unimodal emission, and the light conversion efficiency is low; compared with unimodal emission, the carbon quantum dot with bimodal emission can be controlled, and particularly has wider application prospects in the fields of photoelectric devices (wide luminescence spectrum), ion detection (high accuracy) and the like. Song Jinping et al (CN 109777405A) provide a method for preparing a red-blue dual-emission fluorescent carbon dot, but the emission wavelength of the red-blue dual-emission fluorescent carbon dot does not achieve the aim of controllable tuning; tan Kejun et al (CN 110511751A) use calcein, sodium hydroxide and ethanol solvent to synthesize blue-green double-emission carbon quantum dots by using a solvothermal method, and controllable tuning is achieved by changing the amount of sodium hydroxide or the synthesis time, but strong acid (the pH value of a reaction system is regulated by hydrochloric acid) and strong alkali solution are used in the preparation process, so that secondary pollution is easy to cause, and the wide application of the double-emission carbon quantum dots is greatly limited.
Disclosure of Invention
Based on the method, the invention provides a green preparation method of the adjustable double-emission carbon quantum dots. The method comprises the steps of taking tea leaves as a carbon source, taking ethanol and water as mixed solvents, preparing carbon quantum dots by a hydrothermal synthesis method, wherein the prepared carbon quantum dots have two emission peaks in an excitation range of 350-450nm, and respectively positioned in a blue-green wave band and a red wave band; the adjustable and controllable dual-peak emission intensity can be realized by simply changing the water content in the mixed solvent. The method has the characteristics of green and environment-friendly process, no toxicity, low cost, simple operation and the like, and can be widely applied to the fields of photoelectric devices, ion detection, temperature sensing and the like.
The method comprises the following specific steps:
a green preparation method of a regulatable double-emission carbon quantum dot comprises the following steps:
(1) Grinding tea into powder, extracting with absolute ethanol as extraction solvent, filtering to remove tea residue, and collecting extractive solution;
(2) Mixing a certain amount of extracting solution with deionized water to make the volume content of the deionized water in the mixed solution be 10% -80%, transferring the mixed solution into a reaction kettle, performing hydrothermal carbonization, and naturally cooling to room temperature after the reaction is finished;
(3) And centrifuging and filtering the obtained product to obtain a double-emission carbon quantum dot solution, and storing the double-emission carbon quantum dot solution at the temperature of 4 ℃ for standby.
The preferable scheme is that the dosage ratio g of the tea to the absolute ethyl alcohol is as follows: ml is 4:100.
Preferably, the reaction condition of the hydrothermal carbonization is that the temperature is 160 ℃ and the reaction time is 3 hours.
The application of the adjustable double-emission carbon quantum dot prepared by the green preparation method in the fields of photoelectric devices and ion detection.
The invention has the following beneficial effects:
according to the method, tea leaves are used as a carbon source, the red-blue double-emission carbon quantum dots are prepared through a simple hydrothermal synthesis method, and the controllable tuning of double-peak emission is realized through simply changing the water content in the mixed solvent. The method has the characteristics of green and environment-friendly process, no toxicity, low cost, simple operation and the like, and has potential application value in the fields of photoelectric devices, ion detection, temperature sensing and the like.
Drawings
FIG. 1 is a transmission electron microscope image of the carbon quantum dots prepared in example 1;
FIG. 2 is a graph of the emission spectrum of the carbon quantum dots prepared in each example under excitation of 410 nm: a-example 1; b-example 2; c-example 3; d-example 4;
FIG. 3 is a graph of emission spectrum of the carbon quantum dots prepared in each example under 365nm excitation: a-example 1; b-example 2; c-example 3; d-example 4;
fig. 4 is a photograph of luminescence of the carbon quantum dots prepared in each example under 365nm ultraviolet lamp irradiation: a-example 1; b-example 2; c-example 3; d-example 4;
FIG. 5 is an ultraviolet-visible absorption spectrum of the carbon quantum dots prepared in examples 2, 5 and 6;
FIG. 6 is a graph showing the emission spectrum of the carbon quantum dots prepared in examples 5 and 6 under 365nm excitation.
Detailed Description
In order to demonstrate the substantial features and significant advances of the present invention, further illustrative embodiments and effects thereof are described with the following examples.
Embodiment one:
(1) Grinding 4g green tea into powder, extracting with 100ml absolute ethanol as extraction solvent, filtering to remove tea residue, and collecting extractive solution; (2) Mixing 10ml of extracting solution with 1.25ml of deionized water, transferring the mixed solution into a reaction kettle with the volume content of the deionized water being 11.1%, carrying out hydrothermal carbonization, setting the reaction temperature to 160 ℃, the reaction time to 3h, and naturally cooling to room temperature after the reaction is finished; (3) And centrifuging and filtering the obtained product to obtain the red-blue double-emission carbon dot solution in the embodiment.
The carbon quantum dot transmission electron microscope image in the embodiment is shown in figure 1, the carbon quantum dots are in quasi-spherical morphology, and the size distribution is between 2 nm and 5 nm; the emission spectrum under 410nm excitation is shown in figure 2a, the emission spectrum shows two spectral bands of green and red, and peak positions are respectively at 517nm and 673 nm; the emission spectrum at 365nm is shown in FIG. 3a, and the emission spectrum shows two spectral bands of blue and red, and the peak positions are respectively at 480nm and 673 nm.
Embodiment two:
the preparation method of the carbon quantum dots in this example is the same as that in example 1, except that the amount of deionized water added in step (2) is 5ml, and the volume content of deionized water is 33.3%.
The emission spectrum of the carbon quantum dot under 410nm excitation is shown in fig. 2b, the emission spectrum shows two spectral bands of green and red, and peak positions are respectively located at 515nm and 673 nm; the emission spectrum of the carbon quantum dot under 365nm excitation is shown in fig. 3b, the emission spectrum shows two spectral bands of blue and red, and peak positions are respectively positioned at 468nm and 673 nm; the ultraviolet-visible absorption spectrum of the carbon quantum dot in this embodiment is shown in fig. 5a, and has an obvious absorption peak at 273nm, which belongs to the characteristic absorption peak of the carbon quantum dot and is pi-pi transition of c=c bond.
Embodiment III:
the preparation method of the carbon quantum dots in this example is the same as that in example 1, except that the amount of deionized water added in step (2) is 8ml, and the volume content of deionized water is 44.4%.
The emission spectrum of the carbon quantum dot under 410nm excitation is shown in fig. 2c, the emission spectrum shows two spectral bands of green and red, and peak positions are respectively located at 515nm and 673 nm. The emission spectrum of the carbon quantum dot under 365nm excitation is shown in fig. 3c, the emission spectrum shows two spectral bands of blue and red, and peak positions are respectively located at 468nm and 673 nm.
Embodiment four:
the preparation method of the carbon quantum dots in this embodiment is the same as that in embodiment 1, except that the amount of deionized water added in step (2) is 40ml, and the volume content of deionized water is 80%.
The emission spectrum of the carbon quantum dot under 410nm excitation is shown in fig. 2d, the emission spectrum shows two spectral bands of green and red, and peak positions are respectively located at 500nm and 673 nm. The emission spectrum of the carbon quantum dot under 365nm excitation is shown in fig. 3d, the emission spectrum shows two spectral bands of blue and red, and peak positions are respectively located at 450nm and 673 nm.
Fifth embodiment:
the preparation method of the carbon quantum dots in the embodiment is the same as that in the embodiment 1, and is different in that tea leaves used in the step 1 are green tea, and black tea is used in the embodiment; the amount of deionized water added in the step (2) was 3.3ml, and the volume content of deionized water was 25%.
The ultraviolet-visible absorption spectrum of the carbon quantum dot in this embodiment is shown in fig. 5b, and there is an obvious absorption peak at 273nm, which belongs to the characteristic absorption peak of the carbon quantum dot and is pi-pi transition of c=c bond. The emission spectrum of the carbon quantum dot under 365nm excitation is shown in fig. 6a, the emission spectrum shows two spectral bands of blue and red, and peak positions are respectively located at 468nm and 673 nm.
Example six:
the preparation method of the carbon quantum dots in the embodiment is the same as that in the embodiment 1, and is different in that the tea used in the step 1 is green tea, and the embodiment uses white tea; the amount of deionized water added in the step (2) was 3.3ml, and the volume content of deionized water was 25%.
The ultraviolet-visible absorption spectrum of the carbon quantum dot in this embodiment is shown in fig. 5C, and has an obvious absorption peak at 273nm, which belongs to the characteristic absorption peak of the carbon quantum dot and is pi-pi transition of c=c bond. The emission spectrum of the carbon quantum dot under 365nm excitation is shown in fig. 6b, the emission spectrum shows two spectral bands of blue and red, and peak positions are respectively located at 490nm and 673 nm.
The above examples of the invention are, of course, merely illustrative of the invention and are not intended to be limiting of the invention in any way. Other variations and modifications will occur to those skilled in the art upon the above-described examples. All embodiments cannot be exemplified in detail here. Obvious changes and modifications which are extended by the technical proposal of the invention are still within the protection scope of the invention.
Claims (4)
1. The green preparation method of the adjustable double-emission carbon quantum dot is characterized by comprising the following steps of:
(1) Grinding tea into powder, extracting with absolute ethanol as extraction solvent, filtering to remove tea residue, and collecting extractive solution;
(2) Mixing a certain amount of extracting solution with deionized water to make the volume content of the deionized water in the mixed solution be 10% -80%, transferring the mixed solution into a reaction kettle, performing hydrothermal carbonization, and naturally cooling to room temperature after the reaction is finished;
(3) And centrifuging and filtering the obtained product to obtain a double-emission carbon quantum dot solution, and storing the double-emission carbon quantum dot solution at the temperature of 4 ℃ for standby.
2. The green preparation method according to claim 1, wherein the dosage ratio g of tea leaves to absolute ethyl alcohol: ml is 4:100.
3. The green preparation method according to claim 1, wherein the hydrothermal carbonization is carried out under the reaction condition that the temperature is 160 ℃ and the reaction time is 3 hours.
4. An application of the adjustable double-emission carbon quantum dot prepared by the green preparation method of any one of claims 1-3 in the fields of photoelectric devices and ion detection.
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|---|---|---|---|---|
| CN109095453A (en) * | 2018-11-06 | 2018-12-28 | 湖南农业大学 | A kind of preparation method of the fluorescent carbon point based on tealeaves and its manufactured fluorescent carbon point |
| CN109777405A (en) * | 2019-02-03 | 2019-05-21 | 山西大同大学 | A kind of red blue pair emits fluorescent carbon points and for detecting Al simultaneously3+And Cu2+The fluorescence analysis method of ion |
| CN111892036A (en) * | 2020-07-10 | 2020-11-06 | 山西大学 | Method for preparing carbon quantum dots by using waste green tea residues and application thereof |
| CN113148978A (en) * | 2020-12-30 | 2021-07-23 | 宁德师范学院 | Method for synthesizing carbon dots by hydrothermal method by taking tea powder as raw material |
| CN113390840A (en) * | 2021-06-12 | 2021-09-14 | 宁德师范学院 | Method for synthesizing carbon dots and detecting copper ions in water body |
| CN114408896A (en) * | 2020-12-30 | 2022-04-29 | 宁德师范学院 | Method for synthesizing fluorescent carbon dots by using tea leaves as carbon source through one-step method and application of method |
| CN114408898A (en) * | 2022-01-24 | 2022-04-29 | 江苏徐淮地区徐州农业科学研究所(江苏徐州甘薯研究中心) | Biomass carbon dots and preparation method and application thereof |
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- 2023-11-13 CN CN202311499447.3A patent/CN117487546A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109095453A (en) * | 2018-11-06 | 2018-12-28 | 湖南农业大学 | A kind of preparation method of the fluorescent carbon point based on tealeaves and its manufactured fluorescent carbon point |
| CN109777405A (en) * | 2019-02-03 | 2019-05-21 | 山西大同大学 | A kind of red blue pair emits fluorescent carbon points and for detecting Al simultaneously3+And Cu2+The fluorescence analysis method of ion |
| CN111892036A (en) * | 2020-07-10 | 2020-11-06 | 山西大学 | Method for preparing carbon quantum dots by using waste green tea residues and application thereof |
| CN113148978A (en) * | 2020-12-30 | 2021-07-23 | 宁德师范学院 | Method for synthesizing carbon dots by hydrothermal method by taking tea powder as raw material |
| CN114408896A (en) * | 2020-12-30 | 2022-04-29 | 宁德师范学院 | Method for synthesizing fluorescent carbon dots by using tea leaves as carbon source through one-step method and application of method |
| CN113390840A (en) * | 2021-06-12 | 2021-09-14 | 宁德师范学院 | Method for synthesizing carbon dots and detecting copper ions in water body |
| CN114408898A (en) * | 2022-01-24 | 2022-04-29 | 江苏徐淮地区徐州农业科学研究所(江苏徐州甘薯研究中心) | Biomass carbon dots and preparation method and application thereof |
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